A topochemical polymerization of a triacetylene has been achieved by the synthesis of a host molecule specifically designed to preorganize a triacetylene dicarboxylic acid guest in accordance with the exacting structural requirements needed for the reaction. Irradiation of the resulting host–guest complex using γ‐rays yields a base‐soluble polytriacetylene polycarboxylic acid (see picture). This study demonstrates the power of supramolecular synthesis as a preparative tool.
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